Sodium Acetate → N-(5-chloropyridin-2-yl)-2-acetoxyacetamide

HRID 1820934

반응식

HRID 1820934 반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][N:7]=1)=[O:4].[C:13]([O-:16])(=[O:15])[CH3:14].[Na+]>CN(C)C=O.C(OCC)(=O)C>[Cl:12][C:9]1[CH:10]=[CH:11][C:6]([NH:5][C:3](=[O:4])[CH2:2][O:16][C:13](=[O:15])[CH3:14])=[N:7][CH:8]=1

참가 물질

5

반응물 2

HCID 517045Sodium AcetateHCID 51511482-chloro-N-(5-chloropyridin-2-yl)acetamide

생성물 1

HCID 23062652N-(5-chloropyridin-2-yl)-2-acetoxyacetamide수율 89.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

2-Chloro-N-(5-chloropyridin-2-yl)acetamide (30.68 g) obtained in Reference Example 26(1) is dissolved in N,N-dimethylformamide (500 ml), thereto is added sodium acetate (24.55 g), and the mixture is stirred at 60° C. for 5 hours. The reaction solution is diluted with ethyl acetate, washed successively with water and saturated brine. The solution is dried over magnesium sulfate, treated with activated charcoal, and the filtrate is concentrated under reduced pressure. The resulting residue is suspended in n-hexane and crystals are collected by filtration, washed with n-hexane, and dried to give N-(5-chloropyridin-2-yl)-2-acetoxyacetamide (30.58 g). APCI-MS M/Z:229/231[M+H]+

후처리

  1. washwashed successively with water and saturated brine
  2. dry with materialThe solution is dried over magnesium sulfate
  3. additiontreated with activated charcoal
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. filtrationcrystals are collected by filtration
  6. washwashed with n-hexane
  7. customdried

출처 및 근거

ORD 기록
ord-69929170c9814fa581953b4d1a5fee46
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07605158B2

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